# 1 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" ;cbcaconhse.fa ;3D CBCA(CO)NH - Gradient enhanced. ;Grzesiek and Bax, J. Am. Chem. Soc., 114, 6291-6293 (1992) ;Muhandiran and Kay, J. Magn. Reson. B 103, 203-216 (1994) ;Bruker Avance/Xwin-nmr version ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ;Documentation modifications by Greg Zornetzer (gaz@nmrfam.wisc.edu) ; ; $Id: cbcaconhse.fa,v 1.2 1999/08/01 08:11:04 abild Exp abild $ ; ; Disclaimer: This pulse program is provided "as is" for your ; information. Support for the use of this pulse program is only ; provided to users of the National Magnetic Resonance Facility ; at Madison (NMRFAM). Users of this pulse program employ it at ; their own risk. Neither NMRFAM or University of Wisconsin-Madison ; are liable for any physical or other damage incurred during the ; use of this pulse program. ; ;f1: 1H, f2: 15N, f3: 13C (channel assignments may be changed below) ;o1p: 4.7 ppm 1H ;o2p: 118 ppm 15N ;o3p: use fq3list facbcaconh.C: Cab,Ca (43ppm, 56ppm) 13C ; ;d1: relaxation delay=d1+0.1s ;p1: 90 H1 at pl1 ;pl1: 1H high power ;p2: 90 N15 at pl2 ;pl2: 15N high power ;p3 90 Cab at pl3 (for 90 Cab: sqrt15) ;pl3: 90 Cab (sqrt15) power level ;p6 90 for 180 Cab at pl6 (for 180 Cab: sqrt3) ;pl6 180 Cab sqrt3 power level ;p4 90 Ca at pl4 (sqrt15) ;pl4 90 Ca (sqrt15) power level ;SEDUCE1 pulse shape at power sp5, offset CO-Cab ;p5 180 CO seduce pulse carrier@Cab ;sp5 180 CO seduce power carrier@Cab ;spoal5 Shaped pulse phase offset = 0.5 ;spoff5 CO-Cab = 132 ppm (16600 on 500i) ;spnam5 seduce1 ; ; ;p7 90 CO/CA square shaped pulse sqrt(15) ;sp7 90 CO/CA square shaped power sqrt(15) ;spnam7 fasqua.256 ;spoal7 Shaped pulse phase offset : 0.5 ;spoff7 CO-CA = 119 ppm (15030 Hz on 500i) ; ; ;p8 180 CO/CA square shaped pulse sqrt(15) ;sp8 180 CO/CA square shaped power sqrt(15) ;spnam8 fasqua.256 ;spoal8 Shaped pulse phase offset : 0.5 ;spoff8 CO-CA = 119 ppm (15030 Hz on 500i) ; ; ;H1 Waltz-16x or DIPSI-2x (cpdprg1), using p90 (PCPD1) at pl11 ;cpdprg1: waltz16 ;pcpd1 1H decoupling pulse ;pl11 1H decoupling power ; ;N15 Waltz-16 (cpdprg2), using p90 (PCPD2) at pl12 ;cpdprg2: waltz16 ;pcpd2: 15N decoupling pulse ;pl12 15N decoupling power ; ;Ca SEDUCE1 decoupling of Ca, using pcpd3 at sp3, ; shape seduce1 offset 0, cpdprg3 waltz16sp3. ;cpdprg3: waltz16sp3 ;pcpd3: on-res seduce decoupling of CA pulse ;sp3: on-res seduce deoucpling of CA power ;spnam3: seduce1 ;spoal3: Shaped pulse phase offset: 0.5 ;spoff3: 0 (for on-resonance) ; ; ;N15 evolution: ; in10=in30, SW(N)=1/2*in10 ; l4 complex points; max. is (d10/in10)+1 ; Process as Echo-AntiEcho ; N15 chemical shift axis is reversed: set reverse to true. ;l4: 15N complex points = td2/2 ;in10: 15N evolution increment, SW(N)=1/(2*IN10) ;in30: set equal to in10 ; ; ;C13 evolution: ; in0=in20, SW(C)=1/2*in0 ; l6 complex points, max. is (d20/in20)+1 ; Process as States (although data is acquired as States-TPPI) ;l6 13C complex points = td1/2 ;in0 13C evolution increment: SW(C)=1/(2*in0) ;in20 must be = in0 ;ns=4, 8, ..., ds=4, 8, ... ; ;Recommendations for gradients, triple-axis (single-axis): ;gpz1: 12% ;gpz2: 15% ;gpz3: 29% ;gpz4: 29% ;gpz5: 22% ;gpz6: 29% ;gpx7: 54% adjust for magic angle (0%) ;gpz7: 30% (55%) ;gpz8: 12% ;gpz9: 15% ;gpx10: 54% adjust for magic angle (0%) ;gpz10: 30% (55%) ;gpnam1: sine.50 ;gpnam2: sine.50 ;gpnam3: sine.100 ;gpnam4: sine.32 ;gpnam5: sine.100 ;gpnam6: sine.100 ;gpnam7: sine.100 ;gpnam8: sine.50 ;gpnam9: sine.50 ;gpnam10:sine.20 ; ;#define ONE_D ; uncomment for 1D experiment ;#define SHORT_P2 ;uncomment if p8/2 > p2 ;#define OPTIM_P19 ; uncomment if you want to optimize p19 (GRAD11) ; ; the correct expt time (works with XWIN-NMR 2.x) ; ;Define channel assignments: ; ;You shouldn't have to worry about anything beyond this point :-) ; ;sanity checks ; # 142 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" ; aqseq 321 ; define delay DELTA define delay TAUA define delay TAUA2 define delay TAUB define delay TAUC define delay TAUD define delay TAUE define delay TAUF define delay TAUG define delay TAUG8 define delay TAUG9 define delay TC define delay CEN_HN1 define delay CEN_HC1 define delay CEN_CN1 define pulse H1_90 define pulse H1_180 define pulse N15_90 define pulse N15_180 define pulse CAB_90 define pulse CAB_180 define pulse CA_180 define pulse CO_180 define pulse GRAD1 define pulse GRAD2 define pulse GRAD3 define pulse GRAD4 define pulse GRAD5 define pulse GRAD6 define pulse GRAD7 define pulse GRAD8 define pulse GRAD9 define pulse GRAD10 "d11=100m" ;disk i/o "d12=10u" ;power switching etc. "d13=5u" ;just a short delay "d14=60u" ;ip,id etc "d16=300u" ;gradient recovery "d17=50u" ;short gradient recovery "H1_90=p1" "H1_180=H1_90*2" "N15_90=p2" "N15_180=N15_90*2" "CAB_90=p3" "CAB_180=p6*2" "CA_180=p4*2" "CO_180=p8" "CEN_HC1=(CAB_180-H1_180)/2" "CEN_HN1=N15_90-H1_90" # 198 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" ; "GRAD1=500u" "GRAD2=500u" "GRAD3=1.0m" "GRAD4=250u" "GRAD5=1.0m" "GRAD6=1.5m" "GRAD7=3.000m" "GRAD8=500u" "GRAD9=500u" "p19=305u" ; configurable: set to the optimum value on your instrument "GRAD10=p19" "d0=d13" "d20=3.6m-p5-GRAD4-d16-d13-d12" "d10=12.4m" "d30=12.4m-5.5m-d13*2" "d6=H1_90" "d7=N15_90" "d23=d13*2+d12" "d24=p4*2" "TAUA=1.8m" "TAUA2=TAUA-GRAD2-d13" "TAUB=1.1m-p5-GRAD4-d16-d13" "TAUC=3.6m-p5-d13*3-d12*2" "TAUD=4.4m" "TAUE=12.4m" "TAUF=5.5m-GRAD7-d12-d13*2-d16" "TAUG=2.3m" "TAUG8=TAUG-GRAD8" "TAUG9=TAUG-GRAD9" "TC=d20" "DELTA=GRAD10+d16+d13*2" "d31=2*(GRAD2+TAUA2+GRAD4+TAUC+TAUE+GRAD8+TAUG8+GRAD9+TAUG9)+GRAD1+GRAD3+TC+GRAD5+GRAD6+GRAD7+DELTA+GRAD10" # 1 "/u/exp/stan/nmr/lists/pp//Avance.incl" ;Avance.incl ; ;version 99/08/02 # 248 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" # 1 "/u/exp/stan/nmr/lists/pp//Grad.incl" ;Grad.incl - include file for Gradient Spectroscopy ;avance-version ;version 99/02/19 define list EA= # 249 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" 1 ze 2 d13 do:f2 d11 setnmr2^0 d14 d14 3 d14 d14 d14 d14 d14 d14 4 d14 d14 d14 5 d14 d14 d14 d14 6 d13 # 1 "/u/exp/stan/nmr/lists/pp//faexptcorr.incl" ; This is here to trick "expt" to calculate the experiment time ; correctly. if "1 == 1" goto nod31 d31 nod31, d13 # 271 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" d1 pl1:f1 pl2:f2 ;--------------------- carbon freq. on Cab --------------- d14 fq3:f3 d12 pl3:f3 d13 setnmr2|0 d13 setnmr0|34 (CAB_90 ph0):f3 d13 GRAD1:gp1 ;500u, 8G/cm d16 ;--------------------- INEPT to Cab ---------------------- (H1_90 ph0):f1 d13 GRAD2:gp2 ;500u, 8G/cm TAUA2 pl6:f3 (CEN_HC1 H1_180 ph0):f1 (CAB_180 ph0):f3 d13 GRAD2:gp2 ;500u, 8G/cm TAUA2 (H1_90*55 ph0):f1 d13 (H1_90 ph1):f1 d13 GRAD3:gp3 ;1m, 20G/cm d16 pl3:f3 (CAB_90 ph11):f3 ;--------------------- Constant time Cab evolution -------- d0 d12 pl0:f3 (p5:sp5 ph0):f3 (N15_180 ph0):f2 d13 GRAD4:gp4 ;250u, 20G/cm d16 (TC) (TAUB H1_180 ph0):f1 d12 pl6:f3 (CAB_180 ph0):f3 d13 d20 GRAD4:gp4 ;250u, 20G/cm d16 d12 pl0:f3 (p5:sp5 ph0):f3 d13 d12 pl3:f3 ;----------------------- INEPT to f3' --------------------- (CAB_90 ph0):f3 d13 \n d12 pl11:f1 \n d13 cpds1:f1 d12 pl0:f3 (p5:sp5 ph0):f3 d13 TAUC pl6:f3 (CAB_180 ph12):f3 d12 pl0:f3 (p5:sp5 ph0):f3 d13 TAUC pl3:f3 d23 (CAB_90 ph0):f3 d13 do:f1 \n d12 pl1:f1 GRAD5:gp5 ;1m, 15G/cm d17 d13 \n d12 pl11:f1 \n d13 cpds1:f1 ;----------------------- Switch frequency to Ca -------------- d16 fq3:f3 ;----------------------- INEPT to f2 -------------------------- d12 pl0:f3 (p7:sp7 ph13):f3 d13 d12 pl4:f3 (TAUE) (TAUD CA_180 ph0):f3 d12 pl0:f3 d24 (CO_180:sp8 ph0):f3 (TAUE) (N15_180 ph0):f2 d12 pl4:f3 (CA_180 ph0):f3 d13 d12 pl0:f3 (p7:sp7 ph0):f3 d13 do:f1 \n d12 pl1:f1 GRAD6:gp6 ;1.5m, 20G/cm d17 d13 \n d12 pl11:f1 \n d13 cpds1:f1 d16 pl0:f3 d13 \n d12 pl0:f3 \n d13 cpds3:f3 (N15_90 ph14):f2 d10 d13 do:f3 d12 pl0:f3 # 363 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" (CO_180:sp8 ph0):f3 (N15_180 ph15):f2 d13 \n d12 pl0:f3 \n d13 cpds3:f3 d30 d13 do:f1 \n d12 pl1:f1 TAUF d13 do:f3 d13 GRAD7:gp7 ;1.25m, 30G/cm d16 (N15_90 ph16):f2 d6 (H1_90 ph0):f1 d13 GRAD8:gp8 ;500u, 8G/cm TAUG8 (N15_180 ph0):f2 (H1_180 ph0):f1 d13 GRAD8:gp8 ;500u, 8G/cm TAUG8 d7 (N15_90 ph1):f2 (H1_90 ph1):f1 d13 GRAD9:gp9 ;500u, 8G/cm TAUG9 (CEN_HN1 H1_180 ph0):f1 (N15_180 ph0):f2 d13 GRAD9:gp9 ;500u, 8G/cm TAUG9 (H1_90 ph0):f1 DELTA pl12:f2 (H1_180 ph0):f1 d13 GRAD10:gp10*-1*EA ;125u, -+30G/cm d13 d16 setnmr0^34 go=2 ph31 cpds2:f2 # 407 "/u/exp/stan/nmr/lists/pp/cbcaconhse.s" d11 do:f2 wr #0 if #0 zd d13 setnmr2^0 3m igrad EA d14 ip16 d14 ip16 lo to 3 times 2 d14 dd10 d14 id30 d14 ip14 d14 ip14 d14 ip31 d14 ip31 lo to 4 times l4 d14 rd10 d14 rd30 d14 ip11 lo to 5 times 2 d14 id0 d14 dd20 d14 ip31 d14 ip31 lo to 6 times l6 exit ph0=0 ph1=1 ph2=2 ph3=3 ph11=0 ph12=0 2 ph13=0 2 ph14=0 ph15=0 0 2 2 ph16=0 ph31=0 2